Textile conditioning agent



United States Patented Sept. 1Q, 1957 2,805,992 TEXTILE CONDKTHQNENG AGENT Fred Fortess, Summit, N. 3., Conrad Honing, Camber land, Md., and Charles E. Kip, Montciair, N. 5., as signers to Celanese Corporation of New York, N. Y., a corporation of Delaware No Drawing. Appiication March 3d, 1954, Serial No. 419,914

1 Claim. (Cl. 252-83) This invention relates to the treatment of textile materials and relates more particularly to the treatment of filamentary material with conditioning agents.

In the production of textile fabrics from filamentary material having a basis of organic derivatives of cellulose, the filamentary material is customarily subjected to various mechanical processes, such as spinning, twisting, coning, pirning, hanking, carding, combing, Weaving, knitting and the like. It is common practice to provide the filamentary material undergoing such mechanical processing with a coating of a conditioning agent in order to render the material amenable to such processing. The conditioning agents heretofore employed have not been satisfactory, since they have not been suficiently stable to aging, have not adequately eliminated the tendency for the filaments to accumulate static charges, and could not be removed from the filaments, after the mechanical processing, as easily as desired.

Accordingly, an object of this invention is the provision of an improved conditioning agent for the treatment of filamentary materials having a basis of cellulose acetate or other organic derivative of cellulose which will be free from the foregoing and other disadvantages.

A further object of this invention is to provide an irnproved conditioning agent for filamentary material having a basis of an organic derivative of cellulose, which conditioning agent has excellent lubricating properties, excellent antistatic properties and very high stability, and which is easily removed from the filamentary material by scouring with water.

Other objects of this invention will be apparent from the following detailed description and claim.

In accordance with this invention there is provided a conditioning composition particularly adapted for the treatment of filaments of cellulose acetate or other organic derivative of cellulose, which composition comprises mineral oil, a bodied sperm oil, a higher fatty phosphate, a tertiary amine and a nonionic surface active agent.

The mineral oil used in the conditioning agent of this invention is desirably a white mineral oil having a paraffinie or naphthenic base and having a viscosity of about 40 to 100 seconds. This viscosity and those given here inafter are measured in the Saybolt Universal viscosimeter at 100 F.

The bodied sperm oil used inthe composition of this invention is a liquid prepared by blowing sperm oil at an elevated temperature with air until the viscosity of the oil is increased, preferably to a viscosity of about 200 to 600. As is well known, sperm oil is a partially unsaturated ester of a higher fatty acid with a higher fatty alcohol.

The higher fatty phosphate employed in the conditioning liquid of this invention is a partial ester of phosphoric acid and a long chain aliphatic alcohol or mixture of such alcohols, the average number of carbon atoms in the alcohol being at least about 8, e. g. from 8 to 18, preferably about 10 to 13. In this partial ester there are, on the average, about 1 to 2, preferably about 1.5 to 2, higher fatty alcohol radicals per phosphorus atom. The partial ester may be made from a single alcohol, e. g. n-decanol, or from a blend of alcohols containing not more than of any one single alcohol. For example, the blend of alcohols may comprise such alcohols as n-octyl alcohol, 2- ethyl hexanol, octanol-2, diisobutyl carbinol, 3,5,5,-trimethyl hexanol, n-decanol, Z-n-butyl hexanol-l, Z-ethyl octanol-l, 2-n-butyl octanol-l, n-lauryl alcohol, unidecanols and trideconals. Preferably this blend should contain at least one branch chain alcohol, with the branch chain alcohols constituting at least 25% of the weight of the blend and preferably 50%. It is also desirable, for best results, to use primary alcohols. Desirably the higher fatty phosphate is prepared in mineral oil, as by reacting the long chain aliphatic alcohol or blend of alcohols with a dispersion of an ester-forming phosphorus compound, e. g. phosphorus pentoxide, in mineral oil.

The tertiary amine employed in the composition of this invention is basic and forms a salt with the acidic partial higher fatty phosphate. This amine preferably contains a hydroxyl group, e. g. dibutyl ethanolamine, triethanolamine, diethyl ethanolamine or diethanolamine. Other amines, such as dicyclohexylamine or morpholine, may also be used, if desired. Best results have been obtained with dibutyl ethanolamine, whose salts with the partial higher fatty phosphate are highly compatible in the composition. In addition, when dibutyl ethanolamine is employed the viscosity characteristics of the composition are superior. Thus, the viscosity of the composition is considerably lower and the temperature at which the mixture becomes cloudy on cooling is also lower when the amine used is dibutyl ethanolamine.

The nonionic surface active agent employed in the composition of this invention comprises a polyalkylene oxide radical attached to a higher fatty radical. For example, there may be used polyalkylene oxide derivatives, i. e. esters, ethers and N-substituted amides, of long chain fatty materials, such as the polyalkylene oxide derivatives of long chain fatty acids, fatty alcohols and fatty acid amides. These polyalkylene oxide derivatives act as blending agents to improve the compatibility of the amine-phosphate salt with the mineral oil. They also act to aid in dispersing the conditioning composition in water so that it may be applied to the filaments in the form of an aqueous emulsion, if desired, and may be removed readily from the filaments by scouring in water after the composition has served its functions on the filaments. The polyalkylene oxide derivatives may be prepared by reacting the long chain fatty material with ethylene oxide or other alkylene oxide or with a polyalkylene glycol, such as polyethylene glycol. In the latter case, i. e. when a polyalkylene glycol is used as a reactant, the unreacted glycol should be removed from the reaction products, as by washing the products with brine or the like. The length of the polyalkylene oxide chain of the reaction product may be varied over a considerable range, satisfactory results having been obtained with chain lengths of from about 2 to 10 lower alkylene oxide units. The long chain fatty materials should contain from about 12 to 18 carbon atoms, which carbon atoms may be in a straight chain or in a branched chain. Suitable long chain fatty alcohols are, for example, oleyl alcohol, lauryl alcohol and mixed sperm oil alcohols. Suitable long chain fatty acids are, for example, lauric acid, oleic acid and coconut oil acids. Suitable long chain amides are, for example, oleylamide and lauramide. Best results are obtained by using a mixture of the nonionic surface active agents, such as a blend of polyethylene oxide derivatives of long chain alcohols and acids.

The proportions of the ingredients of the composition of this invention are advantageously within the following ranges: mineral oil, about 35 to 55%, preferably 40 to 45%; higher fatty phosphate, about 5 to 30%, preferably 9 to 20%; bodied sperm oil, aboutS to 45%, preferably 15 to 30%; tertiary amine, about 5 to 20%, preferably 7 to 17% nonionic surface active agent, about 10 to 25%, preferably 12 to 20%. The tertiary amine is desirably presentin. a quantitywhich is at'least high enough to neutralize said higher fatty phosphate. For best resuits the amount of the amine is suchtlrat when 2 parts of the composition of this invention. are dispersed in 98 partsof water the pH of the resulting dispersion is 7.0

to 8.5, preferably about 7.5 to 8.. The composition is preferably prepared by adding all of'theother ingredients to the mineral oil, the tertiaryamine being added last.

The viscosity of the conditioning'composition of this invention may be, varied, .las desired depending to some extent on the manner in'which the. composition is to 'be applied to the filaments of cellulose acetate or other organic derivative of cellulose. Thus, when .the'composition is to be ap lied to the filamentswithout dilution, best 4 oil known as Polysperm'300 and having a viscosity or about 300 seconds; (c) 18 parts by weight of a 50-50 mixture of a mixed partial alkyl phosphate and mineral oil, prepared by reacting 1.88 parts by weight of phosphorus pentoxide dispersed in 9 parts by weight of white mineral oil having a viscosity of 50 seconds with 7.12 parts by weight of a mixture of one mole of n-decanol and one mole of mixed alkanols containing an average of 13 carbon atoms obtained by the oxo process for making primary alcohols; (d) 7 parts by Weight of di-nbutyl ethanolamine; and (f) 20 parts by weight of a mixture of equal proportions by weight of the polyethylene oxide monoether of sperm oil alcohol containing 3 mols l of ethylene oxide per mol of sperm oil alcohol and the results are obtained when the viscosity of the, composition. 1

is about 100 to 200 seconds. When the composition is to heap-plied. as an emulsion therein in water the viscosity of the composition can be higher, i. e. from about 200 to 400-seconds or higher. This increase in viscosity may be effected by the use in the composition of a more viscous, less volatile mineraloil, e. g. a mineral oil having a viscosity of 55 to 75 seconds. Of course, the viscosity of the aqueous emulsion is generally much lower than that of the conditioning composition contained therein, since the emulsion generally contains only a minor proportion of the conditioning composition. Thus, the emulsion may "contain up to about 30%, preferably. about 15 to by weight of the composition of this invention, and'have a viscosity of about 50 seconds or less, e.

about 35 to 50 seconds. The aqueous emulsion may be prepared by simply mixing and agitating the condition ing composition with the desired amount of water.

The conditioning composition of this invention may be applied to continuous filaments as they emerge, in the form of la yarn, from the spinning cabinet or metier in which they are formed. Similarly, it may be applied to a tow, or relatively thick bundle, of continuous filaments before said bundle is severed into staple fibers of the desired length, or it may be applied to the staple fibers themselves at any desired stage in the processing of said staple fibers. Generally, the amount of the cornposition applied to the filamentary material is about 2 to 4%, based on the weight of said filamentary material.

The conditioning compositions of this invention, when compared with the conditioning compositions which the prior art customarily uses for the same purpose, show superior stability to aging and oxidation; show smaller change in viscosity when the amount of moisture in the composition is varied; are more easily removed by scouring in Water; show higher antistatic activity; are lighter in color and darken less on aging. The compositions of this invention have excellent lubricating properties; are

' V out and dep'osit on the'appiaratus used for sizing,

The following examples are given tojillustrate this invention further: 7

Example I A conditioning composition, especially suitable for application to'yarns of continuous filaments of cellulose acetate, is prepared by mixing together (a) 35 parts by weight of a white paraflinic mineral oil having a viscosity of'5-0 seconds;;( b) 20 parts by Weight of the bodied sperm not corrosive to black iron vessels; and may be readily and monoester of oleic acid with a polyethylene glycol, which polyethylene glycol has a molecular weight of about 300, said ester being known as Lipal 30W.

plication to continuous filaments that are. to be converted.

into staple fibers, is prepared by mixing together: (a) 15 parts by weight of a white paraffinic mineral oil having a viscosity of 70 seconds; (bt) '6Hparts'by'weight of Polysperm 300; (c). 50 parts by weight of a mixture of a mixed partial alkyl phosphate and mineral oil prepared by reacting 5.2 parts by weight of'phosphorus pentoxide dispersed in 25 parts by weight of whitemineral oil having a viscosity of 70 seconds with 19.8 parts by Weight of a mixture of one mole of an alkanol having ten carbon atoms and one mole ,of an alkanol having 13 carbon atoms, both alcohols prepared by the oxol process; (d) 17 parts by weight of di-n-butyl ethanolamine; (e) and 12 parts by weight of a mixture of. equal proportions of the samepolyethylene oxide monoether of sperm oil alcohol referred to above and Lipal 30W. 7

While this invention has, been described with particular reference to the treatment of filaments composed of cellulose acetate, the conditioning agents of this invention are also applicable to the treatment of filaments of other 7 nylon, polyesters such as polyethylene terephthalate, polymers and copolymers of:acr.ylonitrile, or polymers and copolymers of vinylidene chloride.

It is to be understood that the foregoing detailed description is given merely by way Of illustration and that many variations may; be made-therein Without departing from the spirit of our, invention.

Having described our invention, what we desire to secure by Letters Patent is:

A textile conditioning composition consisting essentially of 35 to 55% of mineral oil; '5. to 45 %-of bodied sperm oil having a viscosity of aboutr200 to'400 seconds; 51to 30% of a partial higher alkyl phosphate containing 1 to 2 alkyl radicals per phosphorusatom'and anaaverage of i about 10 to 13 carbon atoms per alkyl radical; 5 -to20% of dibutyl ethanolamine;, and '10 to .25. a. of a nonionic surface active agent comprising a mixtureof an .alkylne oxide derivative of a higher fatty acid having 12 to 18" carbon atoms and an alkylenenxidederivative of a higher fatty alcohol-having 12 to 18 carbon atoms, the

pH of said composition, when measured .as a 2% dis-' persion thereof in water, being about to .8.5.

References Cited in the file of this patent UNITED STATES 2,182,323 ,f 52,333,770 Dickey et a1,

I Nov. 9,1943 2,676,924 "Fortess et a'l'. 

